CN111318439A - Ultrasonic transducer based on high-Curie-temperature piezoelectric material and preparation method thereof - Google Patents

Ultrasonic transducer based on high-Curie-temperature piezoelectric material and preparation method thereof Download PDF

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CN111318439A
CN111318439A CN202010137112.7A CN202010137112A CN111318439A CN 111318439 A CN111318439 A CN 111318439A CN 202010137112 A CN202010137112 A CN 202010137112A CN 111318439 A CN111318439 A CN 111318439A
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ultrasonic transducer
piezoelectric
curie temperature
matching layer
layer
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赵祥永
王巨杉
方必军
王飞飞
张巧珍
肖俊杰
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Shanghai Normal University
University of Shanghai for Science and Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B06GENERATING OR TRANSMITTING MECHANICAL VIBRATIONS IN GENERAL
    • B06BMETHODS OR APPARATUS FOR GENERATING OR TRANSMITTING MECHANICAL VIBRATIONS OF INFRASONIC, SONIC, OR ULTRASONIC FREQUENCY, e.g. FOR PERFORMING MECHANICAL WORK IN GENERAL
    • B06B1/00Methods or apparatus for generating mechanical vibrations of infrasonic, sonic, or ultrasonic frequency
    • B06B1/02Methods or apparatus for generating mechanical vibrations of infrasonic, sonic, or ultrasonic frequency making use of electrical energy
    • B06B1/06Methods or apparatus for generating mechanical vibrations of infrasonic, sonic, or ultrasonic frequency making use of electrical energy operating with piezoelectric effect or with electrostriction
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
    • C04B35/49Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206Magnesium oxides or oxide-forming salts thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3251Niobium oxides, niobates, tantalum oxides, tantalates, or oxide-forming salts thereof
    • C04B2235/3255Niobates or tantalates, e.g. silver niobate
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3296Lead oxides, plumbates or oxide forming salts thereof, e.g. silver plumbate

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  • Materials Engineering (AREA)
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  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Transducers For Ultrasonic Waves (AREA)
  • Ultra Sonic Daignosis Equipment (AREA)

Abstract

The invention discloses an ultrasonic transducer based on a high-Curie temperature piezoelectric material and a preparation method thereof, and relates to the technical field of ultrasonic transducers. The ultrasonic transducer consists of a piezoelectric material 1, a matching material layer 2, a backing material layer 3, a metal shell 4 and a coaxial cable 5, and the working frequency of the ultrasonic transducer is 1MHz to 100 MHz. A preparation method of a piezoelectric ceramic ultrasonic transducer based on high Curie temperature comprises the following steps: A. testing the material parameters of the piezoelectric ceramic 1 lead magnesium niobate-lead hafnate-titanic acid; and L, characterizing the acoustic performance of the ultrasonic transducer. The piezoelectric coefficient of the ultrasonic transducer is close to 500pC/N, the electromechanical coupling coefficient under the thickness stretching vibration mode is as high as 56.9 percent, and the piezoelectric coefficient has an important effect on improving the bandwidth and the sensitivity of the ultrasonic transducer. The optical fiber can not be easily depolarized in use under the conditions of high energy and higher temperature, and has important application value in the fields of medical imaging, diagnosis and treatment, nondestructive testing and the like.

Description

Ultrasonic transducer based on high-Curie-temperature piezoelectric material and preparation method thereof
Technical Field
The invention relates to the technical field of ultrasonic transducers, in particular to an ultrasonic transducer based on high Curie temperature piezoelectric ceramics (lead magnesium niobate-lead hafnium titanate) and a preparation method thereof.
Background
X-ray imaging, diagnostic ultrasound imaging, magnetic resonance imaging, and Computed Tomography (CT) and are known as four new techniques for modern medical imaging. Among them, ultrasonic imaging diagnosis is popular in the medical community because of its safety and high efficiency. The ultrasonic transducer is a device for realizing the conversion between electrical energy and acoustic energy, and has important application value in the fields of medical imaging, diagnosis and treatment, nondestructive testing and the like.
The ultrasonic transducer mainly comprises a piezoelectric material, a matching material, a backing material, a metal shell, a coaxial cable and the like. The traditional ultrasonic transducer mainly adopts lead zirconate titanate (namely commercial PZT-5H piezoelectric ceramics) and lead magnesium niobate-lead titanate PMN-PT piezoelectric single crystals as main piezoelectric materials, and because the Curie temperature and the temperature stability of the piezoelectric materials of the two systems are not high enough, the piezoelectric materials of the ultrasonic transducer are easy to depolarize in the use process, so that the performance of the transducer is reduced. Meanwhile, the existing ultrasonic transducer mainly employs the vibration modes of length expansion, radial expansion, transverse expansion, thickness shear, thickness expansion and the like, which are related not only to the shape of the piezoelectric material but also to the purity of the vibration mode of the piezoelectric material. Obviously, the ultrasonic transducer prepared by the high-Curie temperature piezoelectric material can be applied to the fields of medical imaging, diagnosis and treatment and the like, nondestructive testing, high-power ultrasound, high-temperature testing and the like. Therefore, the search and search for new piezoelectric materials with high temperature resistance, high energy and high frequency are the technical problems to be solved urgently in the field of ultrasonic transducers.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings in the prior art and provides an ultrasonic transducer based on high-Curie-temperature piezoelectric ceramic lead magnesium niobate-lead hafnate-lead titanate and a preparation method thereof.
The invention relates to a baseThe ultrasonic transducer of the piezoelectric material with the temperature higher than the Curie temperature consists of piezoelectric ceramics, a matching material layer, a backing material layer, a metal shell and a coaxial cable, wherein the piezoelectric ceramics are lead magnesium niobate-lead hafnium titanate ceramics (0.15Pb (Mg)1/3Nb2/3)O3-0.38PbHfO3-0.47PbTiO3) The thickness is 20-1500 μm, the Curie temperature is more than 290 ℃, and the temperature stability is kept from room temperature to 260 ℃.
The matching material layer is a single matching layer or a double matching layer.
The backing material layer is a mixture of epoxy resin and tungsten powder, and the acoustic impedance of the backing material layer is 4Mrayl to 7 Mrayl.
The single matching layer has a frequency range of 10MHz to 100 MHz; the frequency range of the double matching layers is 1MHz to 10 MHz.
The invention relates to a preparation method of an ultrasonic transducer based on a high Curie temperature piezoelectric material, which comprises the following steps:
firstly, testing the material parameters of the piezoelectric ceramic lead magnesium niobate-lead hafnate-lead titanate (0.15PMN-0.38PH-0.47 PT);
secondly, simulating the frequency domain and the time domain of the transducer according to the equivalent circuit KLM model;
thirdly, sequentially mechanically thinning and polishing the piezoelectric ceramics until the thickness is 20-1500 mu m;
fourthly, brushing silver electrodes on the polished piezoelectric ceramics;
fifthly, polarizing the piezoelectric ceramics brushed with the electrodes;
sixthly, casting a backing material layer on one side of the piezoelectric ceramics, and grinding to a set thickness;
seventhly, casting a first matching layer on the other side of the piezoelectric ceramic, and grinding to a set thickness;
eighthly, leading out the core wire on the electrode between the backing material layer and the matching material layer by tin soldering;
ninth, the structure obtained is encapsulated by a metal shell;
step ten, casting a second matching layer on the first matching layer, and grinding to a set thickness;
step ten, connecting the lead wires by using coaxial cables;
and a twelfth step of characterizing the acoustic performance of the ultrasonic transducer.
The piezoelectric coefficient of the piezoelectric material adopted by the ultrasonic transducer is close to 500pC/N, and the electromechanical coupling coefficient in the thickness stretching vibration mode is as high as 56.9 percent, thereby having important function on improving the bandwidth and the sensitivity of the ultrasonic transducer. The material can not be easily depolarized when being used under the conditions of high energy and higher temperature, and has important application value in the industries of medical imaging, diagnosis and treatment and the like, nondestructive testing, geological exploration, oil exploitation, nuclear industry, automobile manufacturing and the like.
Drawings
FIG. 1 is a schematic structural diagram of an ultrasonic transducer based on a high Curie temperature piezoelectric material according to the present invention;
FIG. 2 is a flow chart of a method for manufacturing an ultrasonic transducer based on a high Curie temperature piezoelectric material according to the present invention;
fig. 3 is a time domain and a frequency domain of an ultrasonic transducer designed by a KLM equivalent circuit model according to an embodiment of the present invention;
FIG. 4 is a graph showing the temperature stability of a piezoelectric ceramic according to an embodiment of the present invention;
FIG. 5 illustrates the time domain and the frequency domain of an ultrasonic transducer obtained by practical testing according to an embodiment of the present invention;
fig. 6 shows the sound field performance of the ultrasonic transducer according to the embodiment of the present invention.
Detailed description of the invention
The invention is further described in the following with reference to the figures and examples
The invention relates to a high Curie temperature piezoelectric material based ultrasonic transducer (as shown in figure 1), which consists of piezoelectric ceramics 1, a matching material layer 2, a backing material layer 3, a metal shell 4 and a coaxial cable 5, and is characterized in that the piezoelectric ceramics 1 is lead magnesium niobate-lead hafnate-lead titanate ceramics (0.15PMN-0.38PH-0.47PT), the thickness of the piezoelectric ceramics is 20-1500 mu m, the Curie temperature is higher than 290 ℃, and the temperature stability is kept from room temperature to 260 ℃.
The matching material layer 2 is a single matching layer or a double matching layer.
The backing material layer 3 is a mixture of epoxy resin and tungsten powder, and has acoustic impedance of 4Mrayl to 7 Mrayl.
The side, close to the piezoelectric ceramic 1, of the double matching layer is a first matching layer 2-1, the component of the double matching layer is a mixture of epoxy resin and silicon oxide, and the acoustic impedance is 7Mrayl to 9 Mrayl; the side close to the object to be detected is a second matching layer 2-2, the component of the second matching layer is epoxy resin, and the acoustic impedance is 2Mrayl to 4 Mrayl.
And the single matching layer comprises epoxy resin on the side close to the object to be detected, and the acoustic impedance is 2Mrayl to 4 Mrayl.
The single matching layer has a frequency range of 10MHz to 100 MHz; the frequency range of the double matching layers is 1MHz to 10 MHz.
A method for manufacturing an ultrasonic transducer based on a high curie temperature piezoelectric material (as shown in fig. 2), the embodiment includes the following steps:
A. the material parameters of the lead magnesium niobate-lead hafnate-lead titanate (0.15PMN-0.38PH-0.47PT) piezoelectric ceramics are tested.
B. The transducer was simulated in the frequency and time domains according to the equivalent circuit KLM model (as shown in fig. 3).
C. And sequentially mechanically thinning and polishing the piezoelectric ceramic 1 until the optimal thickness is 1280 mu m.
D. The polished piezoelectric ceramic 1 is brushed with a silver electrode.
E. The piezoelectric ceramic 1 after brushing the electrodes is polarized.
F. Epoxy resin and tungsten powder are mixed according to the proportion of 1: 2 on one side of the piezoelectric ceramic 1, then are stirred uniformly and cast to be used as a backing material layer 3, the acoustic impedance of the backing material layer is 5.4Mrayl, and then are ground flat to the thickness of 8 mm.
G. On the other side of the piezoelectric ceramic 1, epoxy resin and silicon oxide were mixed in a ratio of 1: 4, and then the first matching layer 2-1 was cast with stirring, with an acoustic impedance of 8Mrayl, and then ground flat to a thickness of 0.44 mm.
H. The core wire is drawn out from the electrode between the backing material layer 3 and the matching material layer 2 by soldering.
I. The structure obtained above is encapsulated with a metal case 4.
J. Epoxy resin is fully mixed and dried on the first matching layer 2-1 to cast a second matching layer 2-2, the acoustic impedance of which is 3.1Mrayl, which is ground flat to a thickness of 0.33 mm.
K. The lead wires are connected by a coaxial cable 5.
L. characterizing the acoustic performance of the ultrasonic transducer.
Further, the step D polarization condition: polarizing in silicone oil at room temperature under 25kV/cm electric field, wherein the voltage-increasing time is 900s, the pressure-maintaining time is 600s, and the voltage-decreasing time is 900s (as shown in figure 4).
And the single matching layer has the use frequency ranging from 10MHz to 100MHz, the step J is omitted, and the thicknesses of the backing material layer 3 and the first matching layer 2-1 are adjusted.
Characterization of acoustic performance of the ultrasonic transducer according to step L of the present invention, a time domain plot and a frequency domain plot (as shown in fig. 5) were obtained by a signal generator (5073PR, Olympus, Japan) and an oscilloscope (Agilent54810A Infinium). The sound intensity distribution of the ultrasonic transducer was measured using a sound field tester (Onda, CA 94089, USA) (as shown in fig. 6).
The piezoelectric coefficient of the piezoelectric material adopted by the ultrasonic transducer is close to 500pC/N, and the electromechanical coupling coefficient in the thickness stretching vibration mode is as high as 56.9 percent, thereby having important function on improving the bandwidth and the sensitivity of the ultrasonic transducer. The material can not be easily depolarized when being used under the conditions of high energy and higher temperature, and has important application value in the industries of medical imaging, diagnosis and treatment, nondestructive testing, geological exploration, oil exploitation, nuclear industry, automobile manufacturing and the like.

Claims (9)

1. The ultrasonic transducer based on the high-Curie-temperature piezoelectric material is composed of piezoelectric ceramics (1), a matching material layer (2), a backing material layer (3), a metal shell (4) and a coaxial cable (5), and is characterized in that the piezoelectric ceramics (1) are lead magnesium niobate-lead hafnium titanate ceramics (xPbb (Mg)1/3Nb2/3)O3-yPbHfO3-(1-x-y)PbTiO3);
The matching material layer (2) is a single matching layer or a double matching layer;
the backing material layer (3) is a mixture of epoxy resin and tungsten powder, and the acoustic impedance of the backing material layer is 4Mrayl to 7 Mrayl.
2. An ultrasonic transducer based on a high curie temperature piezoelectric material according to claim 1, characterized in that the piezoelectric ceramic (1) has a thickness of 20 to 1500 μm, a curie temperature greater than 290 ℃, and a temperature stability of from room temperature to 260 ℃.
3. The ultrasonic transducer based on the high curie temperature piezoelectric material according to claim 1, wherein the double matching layer, the side near the piezoelectric ceramic (1), is a first matching layer (2-1) with a composition of a mixture of epoxy resin and silicon oxide, and has an acoustic impedance of 7Mrayl to 9 Mrayl; the side close to the object to be detected is a second matching layer (2-2), the components are epoxy resin, and the acoustic impedance is 2Mrayl to 4 Mrayl;
and the single matching layer comprises epoxy resin on the side close to the object to be detected, and the acoustic impedance is 2Mrayl to 4 Mrayl.
4. The high curie temperature piezoelectric material based ultrasonic transducer of claim 1, wherein said single matching layer has a frequency range of 10MHz to 100 MHz; the frequency range of the double matching layers is 1MHz to 10 MHz.
5. The high curie temperature piezoelectric material-based ultrasonic transducer of claim 1, wherein the vibration mode of the transducer is a thickness extensional vibration mode or a length extensional vibration mode.
6. A preparation method of an ultrasonic transducer based on a high Curie temperature piezoelectric material is characterized by comprising the following steps:
a, testing the material parameters of the piezoelectric ceramic (1) lead magnesium niobate-lead hafnate-lead titanate (0.15PMN-0.38PH-0.47 PT);
b, simulating the frequency domain and the time domain of the transducer according to the equivalent circuit KLM model;
c, sequentially mechanically thinning and polishing the piezoelectric ceramics (1) until the thickness is 20-1500 mu m;
d, brushing silver electrodes on the polished piezoelectric ceramics (1);
e, polarizing the piezoelectric ceramics (1) after brushing the electrodes;
f, casting a backing material layer (3) on one side of the piezoelectric ceramic (1) and grinding to a set thickness;
g, casting a first matching layer (2-1) on the other side of the piezoelectric ceramic (1) and grinding to a set thickness;
h, leading out the core wire on the electrode between the backing material layer (3) and the matching material layer (2) by soldering;
l, packaging the obtained structure by using a metal shell (4);
j, casting a second matching layer (2-2) on the first matching layer (2-1) again, and grinding to a set thickness;
k, connecting the lead wires by using a coaxial cable (5);
l, characterizing the acoustic performance of the ultrasound transducer.
7. The method for preparing an ultrasonic transducer based on a high curie temperature piezoelectric material according to claim 6, wherein the polarization condition of step D is as follows: polarizing in silicon oil at room temperature according to an electric field of 25kV/cm, wherein the voltage rising time is 900s, the pressure maintaining time is 600s, and the voltage reducing time is 900 s.
8. The method for manufacturing an ultrasonic transducer based on a high curie temperature piezoelectric material according to claims 6 and 7, wherein if the single matching layer has a frequency range of 10MHz to 100MHz, step I is omitted and the thickness of the backing material layer (3) and the first matching layer (2-1) is adjusted.
9. The method for preparing an ultrasonic transducer based on a high curie temperature piezoelectric material according to claims 6 and 7, wherein the step H is implemented by a signal generator (5073PR, Olympus, Japan) and an oscilloscope (Agilent54810A Infinium) to test the time domain and the frequency domain of the ultrasonic transducer and measure the sound intensity distribution curve of the ultrasonic transducer by using a sound field tester (Onda, CA 94089, USA).
CN202010137112.7A 2020-03-02 2020-03-02 Ultrasonic transducer based on high-Curie-temperature piezoelectric material and preparation method thereof Pending CN111318439A (en)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN113182157A (en) * 2021-04-27 2021-07-30 之江实验室 Flexible piezoelectric ultrasonic transducer

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CN113182157A (en) * 2021-04-27 2021-07-30 之江实验室 Flexible piezoelectric ultrasonic transducer

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